固相萃取-液质联用测定辣椒粉中苏丹红

该试验建立了分子印迹固相萃取-超高效液相色谱-串联质谱法检测辣椒粉中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ的方法。辣椒粉样品经过正己烷提取,氮吹浓缩,苏丹红专用分子印迹固相萃取柱净化和富集,以体积分数为0.2%的甲酸水溶液和乙腈为流动相梯度洗脱,经Agilent ZORBAX Eclipse Plus C₁₈(2.1 mm×50 mm,1.8μm)柱分离,ESI+电喷雾模式扫描,MRM多反应模式监测,外标法定量。结果显示,该方法下4种苏丹红的检出限均为5μg/kg,4种化合物在0~50μg/L质量浓度范围内线性关系良好,相关系数均在0.9990以上;当加标浓度为10,50和100μg/kg时,回收率在86.5%~102.2%之间,相对标准偏差均小于6.0%。该方法可为辣椒粉中4种苏丹红的定性定量分析提供参考。

Determination of Sudan Dyes Contents in Chili Powder by SPE-UHPLC-MS/MS

A method was established for the determination of Sudan dyes in chili powder by special solid phase extraction cartridges combined with ultra high performance liquid chromatography-tandem mass spectrometry.The chili powder was extracted with n-hexane,concentrated by nitrogen blowing,purified and enriched by the solid phase extraction cartridges for Sudan dyes.The sample solution was separated by Agilent ZORBAX Eclipse Plus C₁₈ column(2.1 mm×50 mm,1.8μm)with the gradient elution using the mobile phase of acetonitrile-0.2%formic acid in water,detected by the multiple reaction monitoring(MRM)and electrospray mode scanning(ESI+),and qualified by the external standard method.The results showed that the linear correlation coefficients of four kinds of Sudan dyes were all above 0.9990 with 0-50μg/L.The detection limit was 5μg/kg.The recoveries at the level of 10,50 and 100μg/kg were 86.5%-102.2%,and the relative standard deviations were all less than 6.0%.This method could provide a reference for the qualitative and quantitative analysis of four kinds of Sudan dyes in chili powder.